CN109900835A - The device of inorganic constituents and application in a kind of highly sensitive on-line checking cigarette ash - Google Patents
The device of inorganic constituents and application in a kind of highly sensitive on-line checking cigarette ash Download PDFInfo
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Abstract
The present invention is the device of inorganic constituents and application in a kind of highly sensitive on-line checking cigarette ash, and highly sensitive on-line analysis system used includes acidification cigarette ash device, feeder and the highly sensitive detection device of reaction product gas.The application of the highly sensitive on-line analysis is to utilize above-mentioned highly sensitive on-line analysis system, cigarette ash is mixed with the inorganic acid of a certain concentration and volume and carries out acidification reaction, corresponding acids gas is converted by the inorganic constituents in cigarette ash using inorganic acid, then above-mentioned acidification reaction product is carried by the carrier gas that feeder provides certain flow and flows out acidizing device, be finally directly entered the highly sensitive detection device of reaction product gas and analyzed.Flow velocity, cigarette ash dosage, the dosage of inorganic acid and the concentration for changing carrier gas can obtain the acidification reaction product of various concentration, acidification reaction product is directly entered the highly sensitive detection device pre-treatment step of reaction product gas with carrier gas, it is easy to operate, analysis is accurate, detection sensitivity is high, can detect the cigarette ash sample of milligram magnitude.
Description
Technical field
The present invention relates to a kind of device of inorganic constituents in highly sensitive on-line checking cigarette ash and applications, are specifically exactly benefit
Inorganic acid is mixed with the cigarette ash sample of milligram magnitude with the highly sensitive on-line analysis device, is allowed to that acidification reaction acquisition cigarette occurs
The corresponding acids product gas of inorganic constituents in ash, it is highly sensitive that last acids product gas by gas conduit rapidly enters gas
Detection device, to realize the purpose of highly sensitive on-line analysis cigarette ash acidizing product.
Background technique
It is well known that fire not only causes the heavy losses of property that can also cause serious casualties.According to causing fire
The reason of fire can be divided into natural fire and caused fire of artificially setting on fire.It artificially sets on fire and uses some combustion-supporting materials more
Or fire source, common combustion-supporting material has the organic solvents such as diesel oil, gasoline, alcohol and robber cement, and one of fire source of setting on fire is important
Approach is the cigarette lighted, therefore the cigarette ash for effectively distinguishing cigarette ashes and other materials facilitates public security organ's judgement fire class
Type infers cause of fire in turn.Method in document report for analyzing cigarette ash is mainly GC or GC-MS, is usually combined centainly
Offline sample-pretreating method is completed, as organic solvent extractionprocess detects cigarette ash ingredient, and cigarette ash sample size used
It is more.But sample pre-treatments are complicated for operation, and process is cumbersome, it takes time and effort, and the content of cigarette ash contained therein is considerably less,
False negative result is easily caused, thus the accuracy of impact analysis result.
The device and new method for being designed to provide inorganic salts ingredients in a kind of highly sensitive on-line analysis cigarette ash of this paper.It should
Method is the ejector of acidizing product gas so that acidification reaction place of the sample bottle as inorganic salts, Double-channel puncture device is commercialized,
Certain density phosphoric acid and the cigarette ash sample of milligram magnitude are in this hybrid reaction, and then it is high to enter reaction product gas for acidizing product gas
Sensitive detection mechanism is based on vacuum UV lamp using acetone to carry out ionization analysis in the negative ionization mass spectrometer of adjuvant.The party
Method efficiently solves the deficiency of above-mentioned analysis method, realizes highly sensitive on-line analysis, do not need any pre-concentration, derivatization or
Elution step provides a kind of simple and quick, accurate sensitive on-line checking means for inorganic constituents in cigarette ash in research fire
And authentic data.In addition, the device gas circuit is simple, and it is low in cost, convenient for operation.
Summary of the invention
The object of the present invention is to provide a kind of device of inorganic constituents in highly sensitive on-line checking cigarette ash and applications.
The device of inorganic constituents in a kind of highly sensitive on-line checking cigarette ash, it is characterised in that: including closed acidified sample
Bottle, Double-channel puncture device, inorganic acid syringe, magnetic stirring apparatus, feeder and using vacuum UV lamp as the reaction of ionization source
The highly sensitive detection device of product gas；
The closed acidified sample bottle opening is equipped with the silica gel bottle stopper for sealing bottleneck, inorganic acid syringe needle
Inorganic acid can be injected in acidified sample bottle across silica gel bottle stopper, acidified sample bottle built-in magnetic stirrer, under acidified sample bottle
Side is equipped with the magnetic stirring apparatus for heating and stirring acid solution and cigarette ash mixture, mixes for acid solution and the abundant of cigarette ash mixture
It closes and the abundant volatilization of acidification gaseous product is overflowed；
The feeder includes the first, second, third carrier gas gas source, is inserted with Double-channel puncture device beyond the Great Wall in silica gel bottle；
The gas of first carrier gas gas source is passed through in acidified sample bottle through the first mass flowmenter and Double-channel puncture device；
Third carrier gas gas source is passed directly into the highly sensitive detection of reaction product gas as blowback air through third mass flowmenter and fills
In the ionized region at close ion outlet set；
The entrance of tail gas discharging pipe is disposed adjacent to the ionized region side at vacuum UV lamp, the outlet of tail gas discharging pipe and big
Gas phase connects；
Blowback air of the gas vent of acidified sample bottle through sample gas ingress pipe Yu the highly sensitive detection device of reaction product gas
Ionized region between outlet and the entrance of tail gas discharging pipe is connected；
Sample bottle of the carrier gas through the second mass flowmenter and equipped with acetone dopant in second carrier gas gas source is passed through reaction
In ionized region between the outlet of product gas sample product gas ingress pipe and the entrance of tail gas discharging pipe.
The Double-channel puncture device be the tapered tip in lower end cylinder, the upper end Yu Zhuti to have as carrier gas import
Two through-holes in channel and gas export channel, carrier gas introduction channel are through the hollow logical of Double-channel puncture device upper and lower ends
Road, upper open end are carrier gas inlet, are tightly connected with mass flowmenter, and the lower open end at cone point is carrier gas
Outlet；
The gas export channel lower open end is located on the side wall of cylinder as reaction product gas entrance, upper open end
For the outlet of reaction product gas, the outlet of reaction product gas is tightly connected with sample gas ingress pipe；
The reaction product gas entrance in gas export channel is located at the carrier gas outlet top of carrier gas introduction channel, to guarantee
Acidizing product gas is sufficiently carried the entrance that channel is exported by gas by carrier gas；
The lower end of the Double-channel puncture device is placed in the top of acid solution and cigarette ash mixture, in order to avoid encounter magnetic stirrer,
Influence mixing effect.
The Double-channel puncture device and acidified sample bottle by the grafting of silica gel bottle stopper, the carrier gas inlet of carrier gas introduction channel and
The reaction product gas outlet that gas exports channel is located at the outside of acidified sample bottle, carries out by the elasticity of silica gel bottle stopper itself close
Envelope, can effectively prevent the spilling of acidizing product gas, Double-channel puncture device can be removed from acidified sample bottle, and acidified sample bottle
It is adjustable, convenient for holding the inorganic acid of different volumes.
Carrier gas gas source is steel cylinder or purified dry air equipped with oxygen, is equipped with mass flow on carrier gas ingress pipe
Meter, carrier gas flux are controllable.
The highly sensitive detection device of reaction product gas is the analytical equipment of direct gas sampling, predominantly acetone dopant
The negative ion mode on-line mass spectroscopy instrument of the gas sampling based on vacuum UV lamp of auxiliary passes through sample gas ingress pipe and acidification sample
Product bottle is connected, the direct sampling analysis of acidizing product gas taken out of to carrier gas.
The acetone dopant steam brings the electricity of the highly sensitive detection device of reaction product gas by the carrier gas of certain flow
From area, the concentration level of acetone dopant can be adjusted by adjusting flow rate of carrier gas and the volatile quantity of acetone unit time；
The third carrier gas gas source is adjusted by mass flowmenter, be can get the blowback air of certain flow, is led by carrier gas
Pipe enters ionized region, for the humidity of dilute sample gas, and prevents the soot particulates in sample gas from blocking junior's transmission structure
Micropore (through-hole on Skimmer plate).
It is operated, is included the following steps: using any described device in claim 1-6
A. accurate weighed cigarette ash sample is put into acidified sample bottle, tightens silica gel bottle stopper, guarantees acidified sample as possible
Bottle inner sidewall ash-free adherency；
B. a certain amount of inorganic acid is injected in acidified sample bottle using inorganic acid syringe, opens magnetic stirring apparatus, and
Heating temperature is set, heating and stirring state is opened；
C. Double-channel puncture device is connected with the highly sensitive detection device of reaction product gas using sample gas ingress pipe；
D. Double-channel puncture device is inserted into acidified sample bottle, while using the highly sensitive detection device of reaction product gas to acidification
The acidification reaction product on-line sampling analysis of sample bottle outflow, obtains the feature spectrogram of inorganic constituents in cigarette ash.
The Double-channel puncture device is organic polymer or stainless steel material；
The inorganic acid is not volatile low concentration inorganic acid, prevents high volatile high concentrated acid to inorganic salts ingredients
The corrosion of oxidation and ionized region components.
The highly sensitive detection device of reaction product gas is the negative ion mode on-line mass spectroscopy instrument of gas sampling, using vacuum ultraviolet
The photon of lamp transmitting ionizes acetone, obtains high yield electronics, and electronics is captured to obtain oxygen anion, oxygen by the oxygen in carrier gas
Gas anion can be strong to electron affinity energy acids carry out it is effectively ionized, to obtain its feature spectrogram.
Wherein inorganic salts it is acidified reaction obtain corresponding inorganic acids, due to inorganic acid acid group electron affinity energy compared with
Height, therefore the negative oxygen ion that the ionization mode of the auxiliary of the acetone based on vacuum UV lamp generates is suitable for the effectively ionized of inorganic acid,
Corresponding acid radical anion is typically resulted in after negative ion mass spectrum ionization analysis.
Detailed description of the invention
Fig. 1 is the schematic device of inorganic constituents in highly sensitive on-line checking cigarette ash: 1- acidified sample bottle；2- binary channels is worn
Pierce device；3- inorganic acid syringe；4- carrier gas introduction channel；5- gas exports channel；6- acid solution and cigarette ash mixture；7- magnetic force stirs
Mix son；8- magnetic stirring apparatus；9- sample gas ingress pipe；10,12,18- carrier gas gas sources；11,13,19- mass flowmenters；15- is true
Empty ultraviolet lamp；16- ionized region；17- tail gas discharging pipe；The highly sensitive detection device of 20- reaction product gas.
Fig. 2 is the feature spectrogram of six kinds of different cigarette ashes.
Fig. 3 is the feature spectrogram of five kinds of different fitment material for family ashes.
Specific embodiment
Firstly, Fig. 1 is a kind of device of inorganic constituents in highly sensitive on-line checking cigarette ash, it is characterised in that: including closed
Acidified sample bottle 1, Double-channel puncture device 2, inorganic acid syringe 3, magnetic stirring apparatus 8, feeder and with vacuum UV lamp
15 be the highly sensitive detection device 20 of reaction product gas of ionization source；
Closed 1 opening of acidified sample bottle is equipped with the silica gel bottle stopper for sealing bottleneck, 3 needle of inorganic acid syringe
Head, which passes through silica gel bottle stopper, to inject inorganic acid in acidified sample bottle 1,1 built-in magnetic stirrer 7 of acidified sample bottle, acidified sample
1 lower section of bottle is equipped with the magnetic stirring apparatus 8 for heating and stirring acid solution and cigarette ash mixture 6, for acid solution and cigarette ash mixture 6
Be sufficiently mixed and be acidified gaseous product abundant volatilization overflow；
The feeder includes the first, second, third carrier gas gas source 10,12 and 18, is inserted with bilateral beyond the Great Wall in silica gel bottle
Road puncture outfit 2；The gas of first carrier gas gas source 10 is passed through acidified sample bottle through the first mass flowmenter 11 and Double-channel puncture device 2
In 1；
Third carrier gas gas source 18 is passed directly into the highly sensitive inspection of reaction product gas as blowback air through third mass flowmenter 19
It surveys in the ionized region 16 at the close ion outlet of device 20；
The entrance of tail gas discharging pipe 17 is disposed adjacent to 16 side of ionized region at vacuum UV lamp 15, tail gas discharging pipe 17
Outlet is connected with atmosphere；
The gas vent of acidified sample bottle 1 is anti-through sample gas ingress pipe 9 and the highly sensitive detection device 20 of reaction product gas
Ionized region 16 between flushing air outlet and the entrance of tail gas discharging pipe 17 is connected；
Sample bottle 14 of the carrier gas through the second mass flowmenter 13 and equipped with acetone dopant in second carrier gas gas source 12 is logical
Enter in the ionized region 16 between the outlet of reaction product gas sample product gas ingress pipe 9 and the entrance of tail gas discharging pipe 17.
The Double-channel puncture device 2 is the cylinder at the tapered tip in lower end, and the upper end Yu Zhuti is led as carrier gas to having
Enter two through-holes in channel 4 and gas export channel 5, carrier gas introduction channel 4 is in 2 upper and lower ends of Double-channel puncture device
Empty channel, upper open end are carrier gas inlet, are tightly connected with mass flowmenter 11, the lower open end at cone point
For carrier gas outlet；
Gas export 5 lower open end of channel is located on the side wall of cylinder as reaction product gas entrance, upper opening
End is that reaction product gas exports, and the outlet of reaction product gas is tightly connected with sample gas ingress pipe 9；
The reaction product gas entrance in gas export channel 5 is located at the carrier gas outlet top of carrier gas introduction channel 4, to protect
Acidizing product gas is sufficiently carried the entrance that channel 5 is exported by gas by card carrier gas；
The lower end of the Double-channel puncture device 2 is placed in the top of acid solution Yu cigarette ash mixture 6, in order to avoid encounter magnetic stirrer
7, influence mixing effect.
With acidified sample bottle 1 by the grafting of silica gel bottle stopper, the carrier gas of carrier gas introduction channel 4 enters the Double-channel puncture device 2
The reaction product gas outlet in mouth and gas export channel 5 is located at the outside of acidified sample bottle 1, by the elasticity of silica gel bottle stopper itself
It is sealed, the spilling of acidizing product gas can be effectively prevent, Double-channel puncture device 2 can be removed from acidified sample bottle 1, and acid
It is adjustable to change sample bottle 1, convenient for holding the inorganic acid of different volumes.
Carrier gas gas source is steel cylinder or purified dry air equipped with oxygen, is equipped with mass flow on carrier gas ingress pipe
Meter, carrier gas flux are controllable.
The highly sensitive detection device 20 of reaction product gas is the analytical equipment of direct gas sampling, and predominantly acetone adulterates
Agent auxiliary the gas sampling based on vacuum UV lamp 15 negative ion mode on-line mass spectroscopy instrument, by sample gas ingress pipe 9 with
Acidified sample bottle 1 is connected, the direct sampling analysis of acidizing product gas taken out of to carrier gas.
The acetone dopant steam brings the highly sensitive detection device 20 of reaction product gas by the carrier gas of certain flow
The concentration level of ionized region 16, acetone dopant can be adjusted by adjusting flow rate of carrier gas and the volatile quantity of acetone unit time
Section；
The third carrier gas gas source 18 is adjusted by mass flowmenter 19, be can get the blowback air of certain flow, is passed through load
Airway enters ionized region 16, for the humidity of dilute sample gas, and prevents the soot particulates in sample gas from blocking junior's transmission
The micropore (through-hole on Skimmer plate) of structure.
It is operated, is included the following steps: using any described device in claim 1-6
A. accurate weighed cigarette ash sample is put into acidified sample bottle 1, tightens silica gel bottle stopper, guarantees acidified sample as possible
Bottle 1 inner sidewall ash-free adherency；
B. a certain amount of inorganic acid is injected in acidified sample bottle 1 using inorganic acid syringe 3, opens magnetic stirring apparatus 8,
And heating temperature is set, open heating and stirring state；
C. Double-channel puncture device 2 is connected with the highly sensitive detection device 20 of reaction product gas using sample gas ingress pipe 9；
D. Double-channel puncture device 2 is inserted into acidified sample bottle 1, while right using the highly sensitive detection device 20 of reaction product gas
The acidification reaction product on-line sampling analysis that acidified sample bottle 1 flows out, obtains the feature spectrogram of inorganic constituents in cigarette ash.
The Double-channel puncture device 2 is organic polymer or stainless steel material；
The inorganic acid 9 is not volatile low concentration inorganic acid, prevents high volatile high concentrated acid to inorganic salts ingredients
16 components of oxidation and ionized region corrosion.
The highly sensitive detection device 20 of reaction product gas is the negative ion mode on-line mass spectroscopy instrument of gas sampling, using vacuum purple
The photon that outer lamp 15 emits ionizes acetone, obtains high yield electronics, electronics by the oxygen in carrier gas capture to obtain oxygen bear from
Son, the acids progress that oxygen anion can be strong to electron affinity energy is effectively ionized, to obtain its feature spectrogram.
Wherein, acidified sample bottle is using commercialization 20ml Brown Glass Brown glass bottles and jars only, the outer diameter of Double-channel puncture device about 5mm, material
For polyetheretherketonematerials materials.In addition, gas conduit is all made of the polyfluortetraethylene pipe of outer diameter 4mm, the highly sensitive detection of reaction product gas
The anion time of-flight mass spectrometer that device is assisted using the acetone of vacuum UV lamp ionization, the mass spectrograph are set using orthogonal acceleration
Meter, with the detection of MCP detector, acidification gaseous product enters mass spectrograph by polyfluortetraethylene pipe and is analyzed.It is ionized in experiment
Area's air pressure maintains atmospheric pressure state.
Embodiment 1
For the examination of the device and application performance of inorganic constituents in a kind of highly sensitive on-line checking cigarette ash of the present invention,
Experiment is using six kinds of different cigarette ashes as object, and using the highly sensitive on-line analysis device on-line analysis, their acidification reaction is produced
Object, to determine contained inorganic salts ingredients.The flow for being set into high-purity dry air of acidified sample bottle is 0.1L/min, used
The H that inorganic acid is 3%3PO4, cigarette ash quality is 5mg, and H is added3PO4About 1ml.It is special in view of the high electron affinity energy of inorganic acid acid group
Property, using the vacuum UV lamp ionization of 115ppmv acetone auxiliary, ionized region air pressure maintains the ionization mode of ionization source in experiment
Atmospheric pressure state, blowback gas velocity 1.5L/min.1ml H is added in ash-free before this3PO4Carry out blank test, sampling
Time is 5min.Later, 5mg cigarette ash and 1ml H are added in a clean acidified sample bottle3PO4, it is inserted into Double-channel puncture
It is quickly passed through carrier gas after device and carries out sampling analysis using mass spectrograph immediately.Fig. 2 is the feature spectrogram of six kinds of different cigarette ashes.
Inferred according to the mass number of quasi-molecular ions and relative intensity, the equal inorganic acid characteristic ion peak containing superhigh intensity in six kinds of cigarette ashs
OCN-(m/z=42), HOCN.O2 -(m/z=75) and NO2 -(m/z=46).Above-mentioned quasi-molecular ions be in cigarette ashes inorganic salts at
The feature spectral peak divided, for distinguishing cigarette ashes and other cigarette ash ingredients.
Embodiment 2
For the examination of the device and application performance of inorganic constituents in a kind of highly sensitive on-line checking cigarette ash of the present invention,
Experiment utilizes highly sensitive their acidification reaction of on-line analysis device on-line analysis using five kinds of different fitment material for family ashes as object
Product, to determine contained inorganic salts ingredients.The flow for being set into high-purity dry air of acidified sample bottle is 0.1L/min, institute
The H for being 3% with inorganic acid3PO4, cigarette ash quality is 5mg, and H is added3PO4About 1ml.In view of the high electron affinity energy of inorganic acid acid group
Characteristic, using the vacuum UV lamp ionization of 115ppmv acetone auxiliary, ionized region air pressure maintains the ionization mode of ionization source in experiment
In atmospheric pressure state, blowback gas velocity 1.5L/min.1ml H is added in ash-free before this3PO4Blank test is carried out, is adopted
The sample time is 5min.Later, 5mg ash sample and 1ml H are added in a clean acidified sample bottle3PO4, it is inserted into binary channels and wears
It is quickly passed through carrier gas after thorn device and carries out sampling analysis using mass spectrograph immediately.Fig. 3 is the feature of five kinds of different fitment material for family ashes
Spectrogram.Inferred according to the mass number of quasi-molecular ions and relative intensity, quasi-molecular ions OCN is also contained in five kinds of fitment material for family ash samples-(m/
Z=42), HOCN.O2 -(m/z=75) and NO2 -(m/z=46), but its intensity is obtained well below cigarette ashes acidizing product
Ionic strength.Therefore, above-mentioned quasi-molecular ions can be used as the feature spectral peak of inorganic salts ingredients in cigarette ashes, for distinguishing cigarette ashes
With other fitment material for family ash.
Claims (9)
1. the device of inorganic constituents in a kind of highly sensitive on-line checking cigarette ash, it is characterised in that: including closed acidified sample bottle
(1), Double-channel puncture device (2), inorganic acid syringe (3), magnetic stirring apparatus (8), feeder and with vacuum UV lamp (15)
For the highly sensitive detection device of reaction product gas (20) of ionization source；
Closed acidified sample bottle (1) opening is equipped with the silica gel bottle stopper for sealing bottleneck, inorganic acid syringe (3) needle
Head, which passes through silica gel bottle stopper, to inject inorganic acid in acidified sample bottle (1), acidified sample bottle (1) built-in magnetic stirrer (7), acid
Change the magnetic stirring apparatus (8) being equipped with below sample bottle (1) for heating and stirring acid solution and cigarette ash mixture (6), is used for acid solution
The abundant volatilization for being sufficiently mixed and being acidified gaseous product with cigarette ash mixture (6) is overflowed；
The feeder includes the first, second, third carrier gas gas source (10), (12) and (18), is inserted with beyond the Great Wall in silica gel bottle double
Access penetrations device (2)；The gas of first carrier gas gas source (10) is passed through through the first mass flowmenter (11) and Double-channel puncture device (2)
In acidified sample bottle (1)；
Third carrier gas gas source (18) is passed directly into the highly sensitive inspection of reaction product gas as blowback air through third mass flowmenter (19)
It surveys in the ionized region (16) at the close ion outlet of device (20)；
The entrance of tail gas discharging pipe (17) is disposed adjacent to ionized region (16) side at vacuum UV lamp (15), tail gas discharging pipe
(17) outlet is connected with atmosphere；
The gas vent of acidified sample bottle (1) is through sample gas ingress pipe (9) and the highly sensitive detection device of reaction product gas (20)
Ionized region (16) between blowback air outlet and the entrance of tail gas discharging pipe (17) is connected；
Sample bottle (14) of the carrier gas through the second mass flowmenter (13) and equipped with acetone dopant in second carrier gas gas source (12)
It is passed through in the ionized region (16) between reaction product gas sample product gas ingress pipe (9) outlet and the entrance of tail gas discharging pipe (17).
2. the apparatus according to claim 1, it is characterised in that:
The Double-channel puncture device (2) be the tapered tip in lower end cylinder, the upper end Yu Zhuti to have as carrier gas import
Two through-holes in channel (4) and gas export channel (5), carrier gas introduction channel (4) are through Double-channel puncture device (2) up and down two
The hollow channel at end, upper open end are carrier gas inlet, are tightly connected with mass flowmenter (11), at cone point
Lower open end is carrier gas outlet；
Gas export channel (5) lower open end is located on the side wall of cylinder as reaction product gas entrance, upper open end
For the outlet of reaction product gas, the outlet of reaction product gas is tightly connected with sample gas ingress pipe (9)；
The reaction product gas entrance of gas export channel (5) is located at the carrier gas outlet top of carrier gas introduction channel (4), to protect
Acidizing product gas is sufficiently carried the entrance by gas export channel (5) by card carrier gas；
The lower end of the Double-channel puncture device (2) is placed in the top of acid solution Yu cigarette ash mixture (6), in order to avoid encounter magnetic stirrer
(7), mixing effect is influenced.
3. the apparatus of claim 2, it is characterised in that:
The Double-channel puncture device (2) and acidified sample bottle (1) pass through the grafting of silica gel bottle stopper, the carrier gas of carrier gas introduction channel (4)
Entrance and the outlet of the reaction product gas of gas export channel (5) are located at the outside of acidified sample bottle (1), by silica gel bottle stopper itself
Elasticity be sealed, the spilling of acidizing product gas can be effectively prevent, Double-channel puncture device (2) can be from acidified sample bottle (1)
On remove, and acidified sample bottle (1) is adjustable, convenient for holding the inorganic acid of different volumes.
4. the apparatus according to claim 1, it is characterised in that:
Carrier gas gas source is steel cylinder or purified dry air equipped with oxygen, is equipped with mass flowmenter on carrier gas ingress pipe,
Carrier gas flux is controllable.
5. the apparatus according to claim 1, it is characterised in that:
The highly sensitive detection device of reaction product gas (20) is the analytical equipment of direct gas sampling, predominantly acetone dopant
The negative ion mode on-line mass spectroscopy instrument of the gas sampling based on vacuum UV lamp (15) of auxiliary, passes through sample gas ingress pipe (9)
It is connected with acidified sample bottle (1), the direct sampling analysis of acidizing product gas that carrier gas is taken out of.
6. the apparatus according to claim 1, it is characterised in that:
The acetone dopant steam brings the electricity of the highly sensitive detection device of reaction product gas (20) by the carrier gas of certain flow
From area (16), the concentration level of acetone dopant can be adjusted by adjusting flow rate of carrier gas and the volatile quantity of acetone unit time
Section；
The third carrier gas gas source (18) is adjusted by mass flowmenter (19), be can get the blowback air of certain flow, is passed through load
Airway enters ionized region (16), for the humidity of dilute sample gas, and prevents the soot particulates in sample gas from blocking junior and passes
The micropore (through-hole on Skimmer plate) of defeated structure.
7. a kind of any described device of the claim 1-6 inorganic constituents analytic process in highly sensitive on-line checking cigarette ash is answered
With, it is characterised in that:
It is operated, is included the following steps: using any described device in claim 1-6
A. accurate weighed cigarette ash sample is put into acidified sample bottle (1), tightens silica gel bottle stopper, guarantee acidified sample bottle as possible
(1) inner sidewall ash-free adheres to；
B. magnetic stirring apparatus is opened by a certain amount of inorganic acid injection acidified sample bottle (1) using inorganic acid syringe (3)
(8), and heating temperature is set, opens heating and stirring state；
C. Double-channel puncture device (2) is connected with the highly sensitive detection device of reaction product gas (20) using sample gas ingress pipe (9)；
D. Double-channel puncture device (2) are inserted into acidified sample bottle (1), while utilize the highly sensitive detection device of reaction product gas (20)
Acidification reaction product on-line sampling analysis to acidified sample bottle (1) outflow, obtains the feature spectrogram of inorganic constituents in cigarette ash.
8. application according to claim 7, it is characterised in that:
The Double-channel puncture device (2) is organic polymer or stainless steel material；
The inorganic acid (9) is not volatile low concentration inorganic acid, prevents high volatile high concentrated acid to inorganic salts ingredients
The corrosion of oxidation and ionized region (16) components.
9. application according to claim 7, it is characterised in that:
The highly sensitive detection device of reaction product gas (20) is the negative ion mode on-line mass spectroscopy instrument of gas sampling, using vacuum ultraviolet
The photon of lamp (15) transmitting ionizes acetone, obtains high yield electronics, electronics by the oxygen in carrier gas capture to obtain oxygen bear from
Son, the acids progress that oxygen anion can be strong to electron affinity energy is effectively ionized, to obtain its feature spectrogram.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111122688A (en) * | 2019-11-25 | 2020-05-08 | 应急管理部沈阳消防研究所 | Fire material evidence identification method for cigarette combustion ash |
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